微波消解-电感耦合等离子体质谱(ICP-MS)法测定稀释沥青中23种元素

稀释沥青是一种中间产品，主要用于生产沥青。目前稀释沥青中元素含量的测定方法较少，前处理过程繁琐。本文采用微波消解-电感耦合等离子体质谱法同时测定稀释沥青中铝、钒、铬、锰、铁、钴等23种元素，对研究稀释沥青各元素组成，具有重要意义。通过选择合适的前处理方式，最终采用微波消解稀释沥青，优化样品称样量、消解试剂、赶酸温度，通过引入内标元素对非质谱干扰进行校正，通过调谐优化仪器参数、碰撞反应池He模式、干扰方程、选择合适同位素等手段对质谱干扰进行了校正。样品进行测定时采用45Sc、72Ge、115In、209Bi作为内标元素，对方法的检出限、精密度、准确度等进行考察。在优化的试验条件下，23种元素在一定的质量浓度范围内与其信号强度呈线性关系，标准曲线线性良好，相关系数在0. 9990~1.0000之间，方法的检出限在0.0005~1.02mg/kg之间，方法用加标回收测定回收率，回收率范围在80.0~110.5%之间，对稀释沥青样品平行测定7次，测定值的相对标准偏差在0.47~3.09%之间。利用该方法对进口稀释沥青进行23种元素进行测定，满足国家标准对各项技术指标参数的要求，检出限低，选择性好，结果准确可靠，为稀释沥青类样品中多种元素分析测定提供了新的参考方法。

Determination of 23 Elements in Diluted Asphalt by Inductively Coupled Plasma Mass Spectrometry（ICP-MS） with Microwave Digestion

Diluted asphalt is an intermediate product mainly used for the production of asphalt.At present, there are few methods for determining the element content in diluted asphalt, and the pre-treatment process is cumbersome. In this paper, simultaneously determination of 23 elements was used by Inductively coupled plasma mass spectrometry with microwave digestion , such as aluminum, vanadium, chromium, manganese, iron and cobalt, in the diluted asphalt. By selecting appropriate pre-treatment methods, microwave digestion of diluted asphalt was ultimately used to optimize sample weighing, digestion reagents, and acid driving temperature. Non mass spectrometry interference was corrected by introducing internal standard elements. Mass spectrometry interference was corrected by tuning and optimizing instrument parameters, collision reaction pool He mode, interference equation, and selecting appropriate isotopes. 45Sc, 72Ge, 115In, 209Bi were used as internal standard elements for sample determination, and the detection limit, precision, and accuracy of the method were investigated. Under optimized experimental conditions, 23 elements exhibit a linear relationship with their signal intensity within a certain mass concentration range, with a good linearity of the standard curve and a correlation coefficient of 0.9990 and 1.0000, the detection limit of the method is between 0.0005 and 1.02mg/kg. The recovery rate of the method is determined using spiked recovery, with a recovery range of 80.0 to 110.5%. Seven parallel measurements were conducted on the diluted asphalt sample, and the relative standard deviation of the measured values is between 0.47 and 3.09%. Using this method to determine 23 elements in imported diluted asphalt meets the requirements of national standards for various technical indicators and parameters. The detection limit is low, the selectivity is good, and the results are accurate and reliable. This provides a new reference method for the analysis and determination of multiple elements in diluted asphalt samples.